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GREEN ENGINEERING
&
PROCESS OPTIMIZATION
using Process Intensification Platforms
Madhav SapreCTO
Pi – Process IntensificationMumbai
22-04-2014 Copyright Pi-Process Intensification Experts LLP 1
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Sustainable Development
22-04-2014 2Copyright Pi-Process Intensification Experts LLP
“Development that meets the needs of the present without compromising the ability of future
generations to meet their own needs.”World Commission on Environment and Development (1987)
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12 Principles of Green Chemistry
• 1. Prevent waste rather than treat/clean it up later
• 2. Invoke atom economy
• 3. Design safer chemicals
• 4. Use & generate less toxic substances
• 5. Massively reduce quantities of solvents used
• 6. Design syntheses for energy efficiency
• 7. Renewable feedstock for large scale processes
• 8. Minimize steps in synthesis
• 9. Use of highly-selective catalytic reagents
• 10. Design materials that innocuously degrade
• 11. Real-time monitoring for pollution prevention
• 12. Minimise potential for accidents
P.T. Anastas and J.C. Warner, Green Chemistry: Theory and Practice, Oxford University Press: New York, 1998, p.30
8 out of 12 can be achieved through intensification of processes & flow chemistry.
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12 Design Principles of Green Engineering
• 1. Prevention instead of treatment(of wastes)
• 2. Maximize Efficiency (of mass, energy, space & time)
• 3. Design separation & purification for ↓materials & energy
• 4. Inherent v/s circumstantial use of non-hazardous inputs
• 5. “Output-Pulled “ v/s “Input-Pushed” use of inputs
• 6. Keep-it-Simple ( complexity is an life-long cost attribute!)
• 7. Design GOAL targeted durability (not immortality)
• 8. Target the “need” (not unnecessary capacity/capability)
(“one-size-fits-all” solutions are a design flaw ! )
• 9. Minimize material diversity
(in multicomponent/multiproduct campaigns)
• 10. Integrate material & energy flows
• 11. Design for commercial “after-life”
• 12. Renewable rather than Depleting material & energy inputs
12 out of 12 can be achieved through intensification of processes & flow chemistry.
22-04-2014 Copyright Pi-Process Intensification Experts LLP 4
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Process Intensification
22-04-2014 Copyright Pi-Process Intensification Experts LLP 5
Process Intensification
Reactions
Flow Chemistry
Other Platforms
Unit Operations
Extraction
Distillation
Crystallization
Filtration
Drying
Air Pollution Control - Absorption
Effluent Treatment
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Pi Benefits
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Optimization Innovation
22-04-2014 8Copyright Pi-Process Intensification Experts LLP
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Optimization - Principles
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Path to Optimization
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An established technique for performing reactions under conditions where :
Mixing
Temperature
Pressure &
Reaction Time
are precisely controlled and safely done.
Variables : ● stoichiometry, ● concentration, ● residence-time,
● temperature and ● pressure are easily adjusted and reactions optimized quickly.
Scale-up : nearly linear and usually done by numbering-up
22-04-2014 Copyright Pi-Process Intensification Experts LLP 11
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Flow Chemistry enables GREEN Engineering
22-04-2014 Copyright Pi-Process Intensification Experts LLP 12
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FLOW Reactors -Fast Track to Optimized ProcessesInspite of continuous processes being widespread in the chemical industry, the development of processes for Fine chemicals & APIs has historically been restricted to the centuries-old technique of iterative-batch-reactions.
Pressure to quickly discover & deliver compounds using scalable processes has compelled the synthetic chemists to harness Flow Chemistry techniques.
Commercial FLOW REACTORS are now an easily available & common enabling technology for performing synthesis in the laboratory & plant scale.
Cost benefits (↓size / ↑safety / ↑ energy efficiency / ↑ yield / ↑ purity) of flow reactors are so compelling, that the cost of the reactor is of subordinate interest.
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FLOW ReactorsTECHNOLOGY PLATFORMS
Selection of apt reactor technology platform is most important for better cost benefit realization :-a) HEAT Transfer Area cost -- for Heat Transfer limited processb) Reactor Volume cost -- for Mass Transfer & slow, kinetically limited process
Key types : Pi offers
Micro-reactors / Microchannel reactors
Falling-film micro-reactors - Tubular & “Dynamic-Tubular” flow reactors Spinning Tube-in-Tube reactors Spinning Disk reactors Spinning Disk FUMI reactors Oscillatory Tube/Baffled flow reactors (OBRs) Microwave assisted flow reactors Sonication-assisted flow reactors Multi-cell flow reactors
Aspirator flow reactors, etc. -
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Industrial Scale “Slurry” FLOW Reactors from Pi
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Coflore “ATR” : Dynamic Agitated Tubular Reactor10 L “ATR” replaces a 8000+ L batch reactor with “high solids-slurry”
10 Litre
Ideal for Hydrogenations & Bio-Catalysis, etc.
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Biocatalysis in “Coflore”
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Biocatalysis in “Coflore”
22-04-2014 17Copyright Pi-Process Intensification Experts LLP
Biocatalytic RESOLUTION of DL-AlanineComparison Batch v/s ATR (continuous)
Gilda Gasparini (AM Technology, UK)
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HYDROGENATION in “Coflore”
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EPOXIDATION in “Coflore”
22-04-2014 19Copyright Pi-Process Intensification Experts LLP
Drivers: High atom efficiency, Tims & Energy conservation, high selectivity and virtually no degradation products (impurities)
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Industrial Scale Spinning-Disk FLOW Reactors
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FUMI Spin Disk Spinning Disk Reactor
SpinPro-300
Volume : 300-1000 ml
Output : 10 T / day +
Forced Uniform Molecular Interdiffusion
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Spinning Disk Reactor - Principle
22-04-2014 21Copyright Pi-Process Intensification Experts LLP
“FUMI” (Forced Uniform Molecular Interdiffusion)
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Industrial Spinning Disk Reactor
22-04-2014 22Copyright Pi-Process Intensification Experts LLP
LAB /Small
PLANTREACTOR
1000s Tonnes/YrPLANT
REACTOR
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Industrial ApplicationsReactions in Spinning Disk Reactors
GRIGNARD ReactionSafe, Atom Efficient, v-Low Impurities & Work-up
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Reactions in Spinning Disk Reactors
Halogen /Lithium Exchange
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21 T/yr on a 2.5” Ø (0.2 ml) Disk // 84 T/yr on a 5” Ø (0.8 ml) Disk
Safe, Atom Efficient, v-High selectivity & No Work-up
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14.76 T/yr on a 2.5” Ø (0.2ml) Disk // 60 T/yr on a 5” Ø (0.8ml) Disk
Reactions in Spinning Disk Reactors
Halogen /Lithium Exchange (cascade)Safe, Atom & Time Efficient, v-Low Impurities & Work-up
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Industrial Scale FLOW Reactors from Pi
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PlantriX (Micro-Channel Reactors)
Plantrix (SiC) (cGMP) from the Netherlands
300 to 1500 Tonne/Yr50 to 275 Tonne/Yr
High Corrosion-Resistant Grade SiC (EKasiC from ESK) Very few & “secure” connections – safer operations & maintenance “non-leachable” & “diffusion-bonded” SiC (not brazed or bolted !)
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Reactions
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GRIGNARD Reaction in PlantriXSiC Micro-Channel Reactor
uses ChemtriX PLANTRIX Micro Reactors
made of EKasic® (SiC) in a pharma API
production plant
Grignard Reactions
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NITRATION
Drivers: Control reaction exotherm (runaway, explosive ) for process safetyHigh “mono- nitro” selectivity , high-productivity & GMP production
DSM selected ChemtriX v/s Corning. Reasons: very few and “secure” connections,
“non-leachable” & “diffusion-bonded” SiC (ChemtriX) v/s Glass or “brazed” SiC (Corning)
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• Highly Exothermic– Batch synthesis delayed 2 months for
DSC information
• Batch scale-up problematic– Yield not reproducible– Increased formation of by-product led
to formation of a gum which was difficult to purify
– Batch synthesis required significantly more time than expected STRONG
EXOTHERM onset at 130 ºC (1373 J/g)
Reactions :Nitration (Novartis)
http://dx.doi.org/10.1021/op200055r
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Process
Intensification
of
UNIT
OPERATIONS
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Unit-Ops -- Extraction
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SpinPro SDE-300
Volume : 300 ml
Throughput : 10,000 L / day +
Extremely High Extraction Efficiency
Drivers: Complete product extraction, ideal for recovery of solvents/organics from waste water, high-productivity & GMP equipment
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Unit-Ops -- Distillation
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Reactor
SplitterExtractive
Distillaton
Solvent
Recovery
Methanol
Recovery
Extractor
Azeo
Column
Decanter
Flash
Column
Color
Column
Flash
Column
Water
Water
Heavies
Methyl
Acetate
Water
Catalyst
Methanol
Acetic Acid
Reactor
Column
Impurity
Removal
Columns
Water
Heavies
Acetic Acid
Methanol
Sulfuric
Acid
Methyl
Acetate
Reactive Distillation
Eastman Chemicals
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Unit-Ops -- Intensified Distillation
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HiGee Distillation
30 mt column replaced by a 1.5 mt column for MeOH Distn.
Drivers: v. high vapour-liquid contact surfaces // v. Low reflux ratios //v. Low energy consumption, v. low space requirements
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Unit-Ops -- Absorption
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Pulsed-Jet Dynamic
Waveform Absorber
Drivers: v. high gas-liquid contact surfaces // v. high efficiency //v. low space requirements
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SUMMARIZINGProcess Intensified & Optimized Reaction & Operation Platforms
1. small footprint & low CAPEX ( a major advantage for sterile-processing & clean-room projects at a fraction of the CAPEX usually required)
2. v. small (and so low cost) Utility CAPEX -- due to v low peak-loads
3. v. high heat transfer area/volume ratios
4. discernable design-space -- QbD built-in
5. reproducible consistent quality & yields (impurity profile is more precise)
6. genuine feasibility for application of PAT (Process Analytical Tools)
7. highly flexible ( key equipments can be plug-&-produce )
8. v. high turn-down ratios ( 1000 : 1 times production capacities)
9. High intrinsic safety due to extremely low reaction volumes, low residence times and high degree of temp/pressure control.
10. easy Lab to Plant scalability
We now see equipments giving 10,000 MT/yr at 1 Litre reaction volume !
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It will be interesting to see how the scene unfolds in INDIA ......
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Major Route Design Factors and Their Interactions
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Quality
Safety
Cost
Durability / Robustness
Environmental Impact
Synthesis Process
T.Y.Zhang, Cem.Rev., 2006, 106, 2583.
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WISH YOU A
GREENER TOMORROW
THANK YOU
22-04-2014 37
?
Questions
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Madhav [email protected]